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The Sabatier/Electrolysis (S/E) process is an attractive approach to in situ propellant production (ISPP), and a breadboard demonstration of this process at Lockheed Martin Astronautics funded by JPL performed very well, with high conversion efficiency, and reliable diurnal operation. There is a net usage of hydrogen in the S/E process, and this has been the principal problem for this approach to ISPP.
Herein, high-performance printed all-polymer solar cells (all-PSCs) based on a bulk-heterojunction (BHJ) blend film are demonstrated using PTzBI as the donor and N2200 as the acceptor. A slot-die process is used to prepare the BHJ blend, which is a cost-effective, high-throughput approach to achieve large-area photovoltaic devices. The real-time crystallization of polymers in the film drying process is investigated by in situ grazing incidence wide-angle X-ray scattering characterization. Printing is found to significantly improve the crystallinity of the polymer blend in comparison with spin coating. Moreover, printing with 1,8-diiodooctane as the solvent additive enhances the polymer aggregation and crystallization during solvent evaporation, eventually leading to multi-length-scale phase separation, with PTzBI-rich domains in-between the N2200 crystalline fibers. This unique morphology achieved by printing fabrication results in an impressively high power conversion efficiency of 9.10%, which is the highest efficiency reported for printed all-PSCs. Finally, these findings provide important guidelines for controlling film drying dynamics for processing all-PSCs.
A procedure for the measurement of gas permeability of an anion exchange membrane (AEM). During the course of the electrochemical reaction, low gas permeation of hydrogen and oxygen through the membrane is crucial to run the process efficiently. The gas permeation rate can be measured using (A) pressure permeation cell, (B) electrochemical monitoring cell, (C) microelectrode and (D) in-situ measurement in MEA. The process relies on a chronoamperometric technique to accurately measure the gas permeation rate across the membrane.
The major problems in fabrication of nano-crystal line materials form nano-powders are: (1), coarsening of the initial nano-size grains, (2), insufficient densification (high concentration of pores), and, (3), conversion of diamond into graphite (for diamond-based ceramics). We have developed a novel technique of the synthesis of nano-composite materials applying very high (up to about 10 GPa) pressures. In this technique, one component is pre-compacted and placed next to another having a lower melting point temperature. The whole sample is pressed and the temperature raised above the melting point of the second component, what results in the melt getting pressed into the (nano-size) pores of the compact. Upon subsequent crystallization the melt forms the second nanophase. The process is fast, on the order of seconds, and the temperatures are relatively low what prevents, or at least significantly reduces coarsening of the starting nanophase grains. Also, conversion of diamond into graphite can be prevented. The technique allows for control of the final product properties through a proper selection of (1) the initial compact density and grain size, (2) chemical composition of the source, and (3) the temperature and pressure of the process. The application of the technique to the synthesis of SiC and diamond with Si, Ge, and different metals. Results of the in-situ investigation of the synthesis process by synchrotron X-ray diffraction technique will be presented.
Every year, TMS Magnesium Committee carefully selects a special topic in magnesium (Mg) related research and development not only having the hottest subject from both academic and industrial perspectives but also demonstrating major achievements within this subject. Following last year’s topic on Mg microallying [1], this year’s focus is on in-situ methods and associated techniques in their broad definition spanning from laboratory- to large- scale facilities to process monitoring. The applications of in-situ techniques have a wide spectrum from the analysis of melts and liquid-solid transitions to solid-state phenomena during thermo-mechanical processing and heat treatments to surface interactions with various environments. Therefore, such works are of significant interest to scientists working in the area of Mg alloy development as well as to a much broader audience from both academia and industry. This interest is primarily caused by challenges in the analysis of structure-property relationship in Mg alloys, and even cursory glance of literature reveals sharp increase of publications relevant to this topic recently. For instance, very high reactivity of Mg as well as its well-known propensity to substantially alter structure upon unloading in mechanical testing makes it difficult to understand and thus to simulate correlation between microstructures observed in post-mortem analysis and physical processes during testing or fabrication. However, recent advances in in-situ analysis based on large-scale research facilities such as neutron scattering and synchrotron radiation sources as well as microscopy-based, acoustic emission, and other more traditional techniques allowed significant achievements. Apart from apparent development of relevant experimental techniques, a significant part of this success should also be attributed to increasing accessibility of the facilities and simplification of their use from a user perspective. The selection of articles in this special topic is quite far from comprehensive review covering all aspects of in-situ methods available for metallic materials development. However, this was not the purpose in any case. Instead, this selection is intended to present several studies on Mg alloys and Mg-based composites with the use of in-situ techniques. In addition, it overviews two techniques, ‘Acoustic Emission’ (AE) and ‘Ambient-Pressure X-ray Photoelectron Spectroscopy’ (AP-XPS), that are rather novel to the Mg community. These studies are supposed to give readers representative examples of such techniques potential and to help in navigating the spectrum of modern state-of-the-art analytical methods facilitating the development of Mg alloys. These articles are organized in the order corresponding to typical Mg alloy lifecycle from material preparation and solidification to thermo-mechanical processing and product fabrication to degradation.
Size and shape of a melt pool play a critical role in determining the microstructure in additively manufactured metals. However, it is very challenging to directly characterize the size and shape of the melt pool beneath the surface of the melt pool during the additive manufacturing process. Here, we report the direct observation and quantification of melt pool variation during the laser powder bed fusion (LPBF) additive manufacturing process under constant input energy density by in-situ high-speed high-energy x-ray imaging. We show that the melt pool can undergo different melting regimes and both the melt pool dimension and melt pool volume can have orders-of-magnitude change under a constant input energy density. Our analysis shows that the significant melt pool variation cannot be solely explained by the energy dissipation rate. We found that energy absorption changes significantly under a constant input energy density, which is another important cause of melt pool variation. Our further analysis reveals that the significant change in energy absorption originates from the separate roles of laser power and scan speed in depression zone development. The results reported here are important for understanding the laser powder bed fusion additive manufacturing process and guiding the development of better metrics for processing parameter design.
A process of preparing an E-carbon nanocomposite includes contacting a porous carbon substrate with an E-containing material to form a mixture; and sonicating the mixture to form the E-carbon nanocomposite; where E is S, Se, Se.sub.xS.sub.y, or Te, x is greater than 0; and y is greater than 0.
Large-format additive manufacturing (LFAM) offers several advantages, including high throughput, cost-effective pellet-fed extrusion, and the capability to produce large-scale structures. The main pain points of LFAM include start and stops during the printing process, warpage, long layer times that lead to bead freezing, and bead separation due to shrinkage. These issues can lead to overfill, underfill and buildup of material in different sections of a print. This can lead to hidden defects embedded within the printed layers, or even ultimate failure of the printed structure. This ensures these defects can only be identified through nondestructive testing (NDT) inspection methods after printing, which can be timely and costly. Aligned Vision work specializes in 2D projectors with visual inspection systems and machine learning. Traditionally system is used for composite layup and layup inspections. In this work we used the LFAM system at Oak Ridge National Laboratory to create defect rich samples. The Aligned Vision inspection system then performed in-situ monitoring of the print process after each part was printed. This in-situ vision inspection system was used to develop a layer-by-layer inspection model that looks for overfill, underfill, and the buildup of defects using only a camera-based vision system. This leads to the assurance of high-quality production components.
A fundamental understanding of spatial and temporal thermal distributions is crucial for predicting solidification and solid-state microstructural development in parts made by additive manufacturing. While sophisticated numerical techniques that are based on finite element or finite volume methods are useful for gaining insight into these phenomena at the length scale of the melt pool (100 - 500 µm), they are ill-suited for predicting engineering trends over full part cross-sections (> 10 x 10 cm) or many layers over long process times (> many days) due to the necessity of fully resolving the heat source characteristics. On the other hand, it is extremely difficult to resolve the highly dynamic nature of the process using purely in-situ characterization techniques. This article proposes a pragmatic alternative based on a semi-analytical approach to predicting the transient heat conduction during powder bed metal additive manufacturing process. The model calculations were theoretically verified for selective laser melting of AlSi10Mg and electron beam melting of IN718 powders for simple cross-sectional geometries and the transient results are compared to steady state predictions from the Rosenthal equation. It is shown that the transient effects of the scan strategy create significant variations in the melt pool geometry and solid-liquid interface velocity, especially as the thermal diffusivity of the material decreases and the pre-heat of the process increases. With positive verification of the strategy, the model was then experimentally validated to simulate two point-melt scan strategies during electron beam melting of IN718, one intended to produce a columnar and one an equiaxed grain structure. Lastly, through comparison of the solidification conditions (i.e. transient and spatial variations of thermal gradient and liquid-solid interface velocity) predicted by the model to phenomenological CET theory, the model accurately predicted the experimental grain structures.
A multi-dimensional model of the Resin Transfer Molding (RTM) process was developed for the prediction of the infiltration behavior of a resin into an anisotropic fiber preform. Frequency dependent electromagnetic sensing (FDEMS) was developed for in-situ monitoring of the RTM process. Flow visualization and mold filling experiments were conducted to verify sensor measurements and model predictions. Test results indicated good agreement between model predictions, sensor readings, and experimental data.
A two-dimensional model of the resin transfer molding (RTM) process was developed which can be used to simulate the infiltration of resin into an anisotropic fibrous preform. Frequency dependent electromagnetic sensing (FDEMS) has been developed for in situ monitoring of the RTM process. Flow visualization tests were performed to obtain data which can be used to verify the sensor measurements and the model predictions. Results of the tests showed that FDEMS can accurately detect the position of the resin flow-front during mold filling, and that the model predicted flow-front patterns agreed well with the measured flow-front patterns.
In situ characterization of catalysts gives direct insight into the working state of the material. Here, the design and performance characteristics of a universal in situ synchrotron-compatible X-ray diffraction cell capable of operation at high temperature and high pressure, 1373 K, and 35 bar, respectively, are reported. Its performance is demonstrated by characterizing a cobalt-based catalyst used in a prototypical high-pressure catalytic reaction, the Fischer–Tropsch synthesis, using X-ray diffraction. Cobalt nanoparticles supported on silica were studied in situ during Fischer–Tropsch catalysis using syngas, H 2 and CO, at 723 K and 20 bar. Post reaction, the Co nanoparticles were carburized at elevated pressure, demonstrating an increased rate of carburization compared with atmospheric studies.
Laser metal additive manufacturing technologies enable the fabrication of geometrically and compositionally complex parts unachievable by conventional manufacturing methods. However, the certification and qualification of additively manufactured parts are greatly hindered by the stochastic melt flow instabilities intrinsic to the process, which has not been explicitly revealed by direct observation. Here, we report the mechanisms of the melt flow instabilities in laser powder bed fusion additive manufacturing process revealed by in-situ high-speed high-resolution synchrotron X-ray imaging. Here we identified powder/droplet impact, significant keyhole oscillation, and melting-mode switching as three major mechanisms for causing melt flow instabilities. We demonstrated the detrimental consequences of these instabilities brought to the process, and presented new understanding on the melt flow evolution and keyhole oscillation. This work provides critical insights into process instabilities during laser metal additive manufacturing, which may guide the development of instability mitigation approaches. The results reported here are also important for the development and validation of high-fidelity computational models.
In powder-bed-based metal additive manufacturing (AM), the visualization and analysis of the powder spreading process are critical for understanding the powder spreading dynamics and mechanisms. Unfortunately, the high spreading speeds, the small size of the powder, and the opacity of the materials present a great challenge for directly observing the powder spreading behavior. In this study, we report a compact and flexible powder spreading system for in situ characterization of the dynamics of the powders during the spreading process by high-speed x-ray imaging. The system enables the tracing of individual powder movement within the narrow gap between the recoater and the substrate at variable spreading speeds from 17 to 322 mm/s. The instrument and method reported here provide a powerful tool for studying powder spreading physics in AM processes and for investigating the physics of granular material flow behavior in a confined environment.
Introduction: Over the last decade, our team based out of NASA Ames Research Center has made advances in fluidic technologies to enable laboratory-grade processes in space environments. More recently, we have designed and developed two instruments that utilize sample processing steps to extract and purify organic molecules that are key targets in the search for life. The first instrument targets soluble lipids and hydrocarbons that have been preserved in soil or rock material for millions to billions of years called ExCALiBR (Extractor for Chemical Analysis of Lipid Biomarkers in Regolith). The second instrument called KAMELOT (Kerogen and Macromolecule Extractor Liberating Organics Thermolytically) targets kerogen or insoluble macromolecular material that reside in the residue left behind after solvent extraction. Together, these instruments can be coupled to existing flight sample acquisition and analytical instrumentation (e.g., mass spectrometers) to achieve our overall science goal of identifying molecular patterns and features that are diagnostic of how the organic matter was synthesized, either through biological or non-biological processes.
All HCMM required were processed. Calibrated and atmospherically corrected sea surface temperatures were developed for the Nantucket Shoals and Gulf of Mexico regions. These data were analyzed and the sea surface temperatures along the various transacts were compared with in situ data. The comparisons indicate that there is, on the average, a root mean square difference between the in situ data and the HCMM sea surface temperatures of + or - 1.0 C. The linear correlation coefficient was 0.97.
Intrinsic graphene possesses many outstanding physical and chemical properties, but their full explorations are often hindered by the effects of substrate and/or contamination. The authors employ the ultrahigh vacuum transmission electron microscopy equipped with a residual gas analyzer to in-situ characterize an effective decontamination process on a suspended graphene. Raman spectroscopic spectra further verify the cleanness of the resultant graphene membrane. The authors also present two contrasting growth morphologies of copper nanoparticles obtained on both clean and unclean graphene surfaces and show that the intrinsic growth dynamics can only manifest on the surface without contaminations.
Abstract Silicon carbide (SiC) can be synthesized in a number of different structural forms known as polytypes with a vast array of optically active point defects of interest for quantum information sciences. The ability to control and vary the polytypes during SiC synthesis may offer a powerful methodology for the formation of new material architectures that expand our ability to manipulate these defects, including extending coherence lifetimes and enhancing room temperature operation. Polytypic control during synthesis presents a significant challenge given the extreme conditions under which SiC is typically grown and the number of factors that can influence polytype selection. In situ monitoring of the synthesis process could significantly expand our ability to formulate novel polytype structures. In this perspective, we outline the state of the art and ongoing challenges for precision synthesis in SiC. We discuss available in situ x-ray characterization methods that will be instrumental in understanding the atomic scale growth of SiC and defect formation mechanisms. We highlight optimistic use cases for SiC heterostructures that will become possible with in situ polytypic control and end by discussing extended opportunities for integration of ultrahigh quality SiC materials with other semiconductor and quantum materials.